CN110818032A - Method for growing bismuth vanadate photo-anode on conductive carrier and bismuth vanadate photo-anode grown on conductive carrier - Google Patents
Method for growing bismuth vanadate photo-anode on conductive carrier and bismuth vanadate photo-anode grown on conductive carrier Download PDFInfo
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Abstract
The invention discloses a method for growing a bismuth vanadate photo-anode on a conductive carrier and a bismuth vanadate photo-anode grown on the conductive carrier. The method comprises the following steps: 1) obtaining a bismuth source solution and a bromine source solution; 2) mixing and stirring the bismuth source solution and the bromine source solution uniformly until the bismuth source solution and the bromine source solution are in a transparent liquid state; 3) pouring the mixed solution into a hydrothermal kettle, immersing the conductive carrier into the mixed solution, placing one conductive surface of the conductive carrier obliquely facing the bottom of the hydrothermal kettle for reaction, and cooling, washing and drying after the reaction is finished to obtain a BiOBr photo-anode precursor; 4) and (3) placing the BiOBr photo-anode precursor in a vanadium source water solution for reaction, and after the reaction is finished, cooling, washing and drying to obtain the bismuth vanadate photo-anode growing on the conductive carrier. The bismuth vanadate photo-anode particle structure is compact, and the nano particles can not fall off from the conductive glass carrier after repeated use, and are easy to recover and reuse.
Description
Technical Field
The invention belongs to the field of electrode manufacturing, and particularly relates to a method for growing a bismuth vanadate photo-anode on a conductive carrier and a bismuth vanadate photo-anode grown on the conductive carrier.
Background
In recent years, TiO2Because of the advantages of high photocatalytic activity, stable physicochemical properties, no toxicity and the like, the catalyst becomes the most widely applied PFC photo-anode catalyst at present. However, TiO2The forbidden band width is wide, only ultraviolet light which only accounts for 4% -5% of sunlight can be utilized, and the electron-hole recombination generated by excitation is serious, so that TiO is caused2The catalyst system has a very low utilization of sunlight. To overcome TiO2In view of these shortcomings, researchers have pointed out a variety of approaches including the compounding of semiconductor materials.
The hydrothermal method is a wet chemical method which is completed in a closed container, and is mainly different from other wet chemical methods such as a sol-gel method and a coprecipitation method in temperature and pressure. Compared with sol-gel method and coprecipitation method, it has the advantages of directly obtaining crystal powder without high-temperature sintering, avoiding hard agglomeration of particles, and eliminating grinding and impurities. At present, the hydrothermal method is the most extensive and applicable preparation method of bismuth vanadate. Compared with bismuth vanadate prepared by other chemical methods, the hydrothermal method has various shapes, is adjustable and controllable, and has few limited factors.
Bismuth vanadate has been widely researched due to the fact that the visible light absorption capacity of bismuth vanadate is far greater than that of titanium dioxide, and is a novel photocatalytic semiconductor with development potential, and is commonly used for photocatalytic electrolysis of water to produce hydrogen, generate oxygen and degrade organic matters. Although bismuth vanadate has been widely studied as a novel semiconductor nanomaterial with visible light absorption. However, all the methods for preparing bismuth vanadate are to prepare bismuth vanadate nanoparticles in the form of powder particles or to use the powder particles as powder particlesPhysical methods (such as spraying, spin coating and the like) are fixed on the conductive glass to form an electrode, or an electrodeposition method is used for preparing the bismuth vanadate photo-anode film, so that the method is not favorable for large-scale production and certain pollution can be caused by powder particles, and the method for preparing the bismuth vanadate photo-anode film by directly growing the bismuth vanadate photo-anode film on the conductive glass does not exist. Secondly, the theoretical maximum photocurrent of bismuth vanadate can reach 7.5mA/cm2However, the maximum photocurrent which can be achieved by the pure bismuth vanadate nanoparticles at present is only microampere level, which is far from the theoretical maximum value. Therefore, there is a need to prepare a high performance pure bismuth vanadate photoanode film grown directly on conductive glass.
Disclosure of Invention
The invention aims to solve the problems and provide a high-performance pure bismuth vanadate photo-anode directly grown on conductive glass.
In order to achieve the above object, a first aspect of the present invention provides a method for growing a bismuth vanadate photo-anode on a conductive support, the method comprising the steps of:
1) dissolving a bismuth source in a first organic solvent to obtain a bismuth source solution with the concentration of more than or equal to 0.01mol/L in terms of bismuth ions, and dissolving a bromine source and an optional surfactant in a second organic solvent to obtain a bromine source solution with the concentration of more than or equal to 0.01mol/L in terms of bromine ions;
2) mixing and stirring a bismuth source solution and a bromine source solution uniformly until the bismuth source solution and the bromine source solution are in a transparent liquid state, wherein the molar ratio of bismuth ions to bromine ions in the mixed solution is 1: 0.5 to 2;
3) pouring the mixed solution into a hydrothermal kettle, immersing a conductive carrier into the mixed solution, placing one conductive surface of the conductive carrier obliquely facing the bottom of the hydrothermal kettle, reacting at 140-200 ℃, and cooling, washing and drying after the reaction is finished to obtain a BiOBr photo-anode precursor;
4) and (3) placing the BiOBr photo-anode precursor into a vanadium source water solution with the concentration of more than 0.02mol/L in terms of vanadium ions, reacting at 140-200 ℃, and cooling, washing and drying after the reaction is finished to obtain the bismuth vanadate photo-anode growing on the conductive carrier.
According to the invention, after the preparation is completed, the bismuth vanadate photoanode grows on the electrode preparation substrate with the conductive surface facing to one side of the bottom of the hydrothermal kettle, and preferably deposits on the other side of the conductive carrier are removed.
According to the invention, the bismuth vanadate photoanode prepared by the method has the advantages that the semiconductor nano-particles are tightly combined with the conductive surface of the carrier, and the bismuth vanadate photoanode is not easy to fall off after repeated use.
As a preferable scheme, in the step 4), after drying, the method further comprises: calcining the product at 400-500 deg.c at the heating rate of 2-5 deg.c/min to obtain bismuth vanadate photo anode growing on the conducting carrier. After calcination, the bismuth vanadate photoanode forms a single crystal structure, and the crystallization is firmer.
Preferably, the conductive carrier is at least one selected from the group consisting of conductive glass, nickel foam, carbon paper, carbon felt, and metal foil. Such as conductive glass FTO, conductive glass ITO, and the like.
Preferably, the first organic solvent is ethylene glycol, and the second organic solvent is ethanol and/or acetone.
Preferably, the bismuth source is at least one selected from the group consisting of bismuth nitrate pentahydrate, bismuth chloride and bismuth sulfate.
Preferably, the bromine source is cetyltrimethylammonium bromide and/or potassium bromide.
As a further preferred embodiment, the bromine source is cetyltrimethylammonium bromide and no surfactant is employed. The bismuth vanadate photoanode prepared by the bromine source without using other surfactants is in a nanometer cluster shape, has a monoclinic phase structure, and is a crystal structure with the smallest semiconductor forbidden bandwidth, namely the widest light absorption range, in three crystal phase structures of the bismuth vanadate semiconductor.
Preferably, the surfactant is sodium dodecyl sulfate, and the concentration of the surfactant in the second organic solvent is 0-0.005 mol/L.
According to the invention, when the bromine source is potassium bromide, sodium dodecyl sulfate can be used as a surfactant, and the prepared bismuth vanadate photoanode is polyhedral.
Preferably, the vanadium source is at least one selected from the group consisting of ammonium metavanadate, vanadium pentoxide, vanadium nitrate and vanadyl acetylacetonate.
Preferably, in step 3), the included angle between the conductive carrier and the bottom plane of the hydrothermal kettle is 40-50 degrees, such as 45 degrees.
Preferably, the concentration of bismuth ions in the bismuth source solution is 0.01 to 0.10 mol/L.
Preferably, the concentration of the bromine source solution is 0.01 to 0.10mol/L in terms of bromide ions.
Preferably, the concentration of the vanadium source aqueous solution is 0.02-0.20mol/L in terms of vanadium ions.
The second aspect of the present invention provides a bismuth vanadate photoanode grown on a conductive support prepared by the above method.
The invention has the following advantages:
1. the invention successfully grows the bismuth vanadate on the conductive carrier by a simple and easily obtained method. The traditional method that bismuth vanadate powder is prepared firstly and then a physical method is used is omitted, such as: and fixing bismuth vanadate powder on the conductive glass by a blade coating method, a spin coating method, a spraying method and the like.
2. The bismuth vanadate photo-anode particle structure is compact, nano particles cannot fall off from a conductive glass carrier after repeated use, and meanwhile, the electrode is high in chemical and thermal stability and easy to recover and reuse.
3. The bismuth vanadate photoanode prepared by the method has a visible light absorption range of 520nm, so that the bismuth vanadate photoanode has better light absorption efficiency.
4. The preparation method disclosed by the invention is simple in preparation process, cheap and easily available in raw materials, low in cost, green and environment-friendly, and can be used for large-scale production compared with the traditional method for preparing the bismuth vanadate photo-anode.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
FIG. 1 shows a Scanning Electron Microscope (SEM) image of flower-like bismuth vanadate prepared in example 1 of the present invention.
Fig. 2 shows a schematic diagram of a bismuth vanadate photo-anode prepared in example 1 of the present invention.
Fig. 3 is a schematic diagram showing the light absorption rate of the bismuth vanadate photo-anode prepared in example 1 of the present invention.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Example 1
1. 30mL of each of a 0.075mol/L bismuth nitrate pentahydrate ethylene glycol solution and a 0.075mol/L cetyltrimethylammonium bromide ethanol solution are prepared.
2. Slowly pouring the bismuth nitrate pentahydrate solution into the cetyltrimethylammonium bromide solution, and uniformly stirring for 30min until the mixed solution is in a transparent liquid state.
3. And pouring the prepared 60mL of mixed solution into a hydrothermal kettle, immersing the conductive glass FTO into the mixed solution, placing one conductive surface of the conductive glass FTO to face the bottom of the hydrothermal kettle at an inclination angle of 45 degrees, and sealing.
4. And (3) putting the hydrothermal kettle into a 160 ℃ oven for heat preservation for 2h, naturally cooling the hydrothermal kettle after the reaction is finished, taking out the BiOBr photo-anode precursor, washing the BiOBr photo-anode precursor with deionized water, and naturally drying in a dark place to obtain the BiOBr photo-anode precursor.
5. Preparing 0.15mol/L metavanadate aqueous solution, wherein the process needs to be carried out by keeping the water temperature at 60-80 ℃, and stirring until the aqueous solution is light yellow.
6. And putting the prepared vanadium source aqueous solution and the BiOBr photo-anode precursor into a hydrothermal kettle together. The mixture is heated in an oven to 180 ℃ and kept for 24 h. And after the reaction is completed, naturally cooling the hydrothermal kettle, taking out the bismuth vanadate photo-anode, washing the bismuth vanadate photo-anode for a plurality of times by using deionized water, and naturally drying the bismuth vanadate photo-anode.
7. And (3) putting the bismuth vanadate photoanode into a muffle furnace, heating to 450 ℃ at a heating rate of 2 ℃/min, and keeping for 2h to obtain the bismuth vanadate photoanode growing on the conductive carrier, as shown in figure 2. FIG. 1 is a scanning electron microscope image of the prepared flower-like bismuth vanadate.
Test example
The photo-electrochemical test of the bismuth vanadate photo-anode grown on the conductive carrier prepared in example 1 was carried out, and the results are as follows:
1. a three-electrode system was used: working electrode (photoanode prepared as described above), counter electrode (Pt electrode) and reference electrode (Hg/Hg)2Cl2)；
2. Preparing a mixed aqueous solution of 0.5M potassium dihydrogen phosphate and 1M sodium sulfite as an electrolyte;
3. cutting the prepared photo-anode into electrode slices of 1cm x 1cm, and clamping by using an electrode clamp;
4. inserting all electrodes into electrolyte, and carrying out photoelectrochemical property test;
5. adjusting the electrochemical workstation to a linear volt-ampere scanning mode, setting the initial potential to be-0.6V and the end potential to be 0.7V, and setting the scanning speed to be 10 mv/s;
6. obtaining a curve with the horizontal axis as the external bias voltage and the vertical axis as the photocurrent density, and obtaining the following formula: RHE +0.0591 pH +0.24 conversion of the transverse-axis bias potential to a reversible hydrogen standard electrode, resulting in a photocurrent density of 0.9mA/cm2At a standard external bias of 1.23V.
7. The curve shows the rule that the current density changes along with the change of the external bias voltage, and the position of the open-circuit voltage can also be judged.
Fig. 3 shows a schematic diagram of the light absorption rate of the bismuth vanadate photoanode prepared in embodiment 1 of the present invention, and as can be seen from fig. 3, the flower cluster shape is favorable for light reflection, the visible light absorption of the bismuth vanadate photoanode prepared by the method is 510nm compared with that of the conventional powdery bismuth vanadate nanomaterial, and the visible light absorption range of the bismuth vanadate photoanode prepared by the method reaches 530 nm.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (10)
1. A method for growing a bismuth vanadate photoanode on a conductive support, the method comprising the steps of:
1) dissolving a bismuth source in a first organic solvent to obtain a bismuth source solution with the concentration of more than or equal to 0.01mol/L in terms of bismuth ions, and dissolving a bromine source and an optional surfactant in a second organic solvent to obtain a bromine source solution with the concentration of more than or equal to 0.01mol/L in terms of bromine ions;
2) mixing and stirring a bismuth source solution and a bromine source solution uniformly until the bismuth source solution and the bromine source solution are in a transparent liquid state, wherein the molar ratio of bismuth ions to bromine ions in the mixed solution is 1: 0.5 to 2;
3) pouring the mixed solution into a hydrothermal kettle, immersing a conductive carrier into the mixed solution, placing one conductive surface of the conductive carrier obliquely facing the bottom of the hydrothermal kettle, reacting at 140-200 ℃, and cooling, washing and drying after the reaction is finished to obtain a BiOBr photo-anode precursor;
4) and (3) placing the BiOBr photo-anode precursor into a vanadium source water solution with the concentration of more than 0.02mol/L in terms of vanadium ions, reacting at 140-200 ℃, and cooling, washing and drying after the reaction is finished to obtain the bismuth vanadate photo-anode growing on the conductive carrier.
2. The method of claim 1, wherein the step 4), after drying, further comprises: calcining the product at 400-500 deg.c at heating rate of 2-5 deg.c/min to obtain bismuth vanadate photo anode growing on the conducting carrier.
3. The method of claim 1, wherein,
the conductive carrier is selected from at least one of conductive glass, foamed nickel, carbon paper, carbon felt and metal sheets;
the first organic solvent is ethylene glycol, and the second organic solvent is ethanol and/or acetone.
4. The method of claim 1, wherein the bismuth source is selected from at least one of bismuth nitrate pentahydrate, bismuth chloride, and bismuth sulfate.
5. The method of claim 1, wherein,
the bromine source is hexadecyl trimethyl ammonium bromide and/or potassium bromide;
preferably, the bromine source is cetyltrimethylammonium bromide, and no surfactant is employed.
6. The method according to claim 1, wherein the surfactant is sodium lauryl sulfate and the concentration of the surfactant in the second organic solvent is 0-0.005 mol/L.
7. The method of claim 1, wherein the source of vanadium is selected from at least one of ammonium metavanadate, vanadium pentoxide, vanadium nitrate, and vanadyl acetylacetonate.
8. The method according to claim 1, wherein in the step 3), the included angle between the conductive carrier and the bottom plane of the hydrothermal kettle is 40-50 degrees.
9. The method of claim 1, wherein,
in the bismuth source solution, the concentration calculated by bismuth ions is 0.01-0.10 mol/L;
in the bromine source solution, the concentration of bromide ions is 0.01-0.10 mol/L;
in the vanadium source water solution, the concentration of vanadium ions is 0.02-0.20 mol/L.
10. A bismuth vanadate photoanode grown on a conductive support prepared by the method of any one of claims 1 to 9.
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